CN103627215B - A kind of preparation method of submicron order silicon powder - Google Patents
A kind of preparation method of submicron order silicon powder Download PDFInfo
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Abstract
The present invention is a kind of preparation method of submicron order silica, relates to the preparing technical field of submicron order material. Concrete steps are: first raw material is put into ball mill and grind, after being sieved, material after grinding adds in sand mill taking water or organic solvent as decentralized medium, add one or more dispersants of silane coupler, titanate coupling agent, HMDS to carry out wet grinding simultaneously, again the slurry after grinding is carried out to deironing through pulp deferrization device, slurry after deironing obtains filter cake by press filtration, and the clear liquid obtaining after press filtration can continue to use as decentralized medium. Technique of the present invention is simple, efficiency is high, the low cost of manufacture of product, yield are high, with short production cycle, without reuniting, size is controlled, be applicable to suitability for industrialized production.
Description
Technical field
The invention belongs to non-metal ore advanced processing technical area, relate to a kind of preparation method of submicron order silicon powder.
Background technology
Silicon powder filler, than other common inorganic fillers, shows good mechanical performance, heat resistance, dispersiveness, electrical property etc. In addition, lower than dielectric constants such as talcum powder, aluminium hydroxide, E-glass fibres and have compared with low water absorbable etc. It is widely used in the industries such as CCL, ink, coating, silicon rubber, Electronic Packaging, accurate manufacture. But along with scientific and technological progress, every profession and trade also proposes higher requirement to silicon powder granularity, particularly more and more stronger to the silicon powder demand of the less submicron order of granularity. As at the electronic product such as mobile phone, computer more and more towards short thin light little future development, therefore require CCL sheet material thinner, this also requires the granularity of filler less. At coating industry, the refractive index of silicon metal micro mist (glass dust) is with resin is approaching mostly, therefore also become best transparent filler, so but due to the large in use free settling of micron-sized silicon powder of its density, this also causes the application of silicon powder in clear dope to be subject to certain limitation. Submicron order silicon powder can thoroughly solve the problem of sedimentation in use procedure, also can improve transparency and the feel of product simultaneously, therefore in high-grade clear dope finish paint, has good prospect.
In the use procedure of filler, often need to add solvent, generally speaking filler granularity is less, and specific area is larger, larger to the viscosity influence of system, submicron order filler, even nano-sized filler in use scattering problem be a problem demanding prompt solution.
Produce submicron order silicon powder both at home and abroad and can be divided into Physical and chemical method. Mainly there is complex process in chemical method, granularity is wayward, material manufacturing cost is high, separation difficulty etc. And Physical can be divided into dry grinding and wet grinding. Dry grinding advantage is that grinding efficiency is high, and product yield is high, but its shortcoming is that classifying equipoment is had relatively high expectations, and general classifying equipoment seldom can reach requirement. Wet grinding milling apparatus is mainly ball mill, but the subject matter that it exists is that grinding efficiency is low, and product yield is low, and the easy reunion of product etc. As patent CN102120581 adopts secondary wet process to grind to prepare ultra-fine torispherical silicon powder taking konilite as raw material, the shortcoming of this method is that to adopt ball mill wet grinding to prepare the energy consumption of super-fine silicon micro-powder higher, in addition prepare material particle size-2 μ m >=97%, granularity does not reach submicron order yet.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, provides that a kind of technique is simple, efficiency is high, cost of goods manufactured is low, yield is high, with short production cycle, size is controlled, without the preparation method of reunion submicron order silicon powder.
Technical problem to be solved by this invention is to realize by following technical scheme. The present invention is a kind of preparation method of submicron order silica, is characterized in, its step is as follows:
(1) dry grinding: choosing granularity is that 2-40 object crystal quartz or vitreous silica sand are raw material, adds in horizontal ball mill, carries out dry grinding taking alumina balls, silicon ball or zirconia ball as mill is situated between; Material after grinding sieves through screen cloth; The diameter that mill is situated between is 10-50mm; The order number of screen cloth is 200-300 order; The mass ratio that when grinding, raw material and mill are situated between is 1:1-4, and milling time is 8-10 hour;
(2) wet grinding: after the material that screening is obtained and decentralized medium, dispersant, add in horizontal sand mill, carry out wet grinding taking alumina balls, carborundum ball or zirconia ball as mill is situated between, mill Jie diameter is 0.2-1.0mm; Described decentralized medium is selected from one or more in water, ethanol, acetone, butanone, and the mass ratio of decentralized medium and material is 3-7:7-3; Described dispersant is selected from one or more of titanate coupling agent, silane coupler, HMDS, the 2-6 ‰ that the addition of dispersant is material; Wet grinding is to slurry granularity D50=0.3-1.0 μ m, D100≤2.0 μ m;
(3) deironing: the slurry after wet grinding is carried out to deironing through duct type pulp deferrization device.
(4) press filtration: the slurry after deironing is obtained to filter cake through press filtration, to obtain final product.
In the preparation method of submicron order silica of the present invention, further preferred technical scheme or technical characterictic are as follows:
1. the supernatant obtaining after step (4) press filtration continues to recycle as decentralized medium, can economize in raw materials like this.
2. after filter cake fragmentation step (4) being obtained, after adding the described decentralized medium of step (2) to mix, ultrasonic wave disperses, and obtains the silica slurry of submicron order, nothing reunion; The mass ratio of filter cake and decentralized medium is 1:1-5, ultrasonic dispersion disposed slurry granularity D50=0.3-1.0 μ m, D100≤2.0 μ m.
3. ultrasonic wave disperses equipment used to be preferably the supersonic wave cleaning machine with agitating device, or ultrasonic wave separating apparatus, hyperacoustic frequency >=25HZ.
4. in step (1), the equipment of screening is vibratory sieve or drum sieve, can be also other screening plant.
5. the liner of the horizontal sand mill described in is aluminium oxide, zirconia or carborundum.
6. the magnetic intensity of the duct type pulp deferrization device that step (3) deironing is used is 8000-15000 Gauss, and the throughput of slurry is 1-5t/h.
7. step (4) press filtration equipment used is box diaphragm filter press.
Compared with prior art, the inventive method technique is simple, and production efficiency is high, the low cost of manufacture of product, yield are high, with short production cycle, and size is controlled, without reuniting. The inventive method had both been produced submicron order silicon powder, had solved again the in use problem of dispersiveness of submicron order silicon powder, and product can be widely used in the industries such as CCL, high-end transparent clear dope finish paint, sapecial coating, ink.
Detailed description of the invention
Below in conjunction with instantiation, the present invention will be further described, below example be not limited to protection scope of the present invention, so to example of the present invention and improve all in protection scope of the present invention.
Embodiment 1, a kind of preparation method of submicron order silica, its step is as follows:
(1) dry grinding: choosing granularity is that 2-40 object crystal quartz or vitreous silica sand are that raw material adds in horizontal ball mill, carries out dry grinding taking alumina balls, silicon ball or zirconia ball as mill is situated between; Material after grinding sieves through screen cloth; The diameter that mill is situated between is 10-50mm; The order number of screen cloth is 200-300 order; The mass ratio that when grinding, raw material and mill are situated between is 1:1, and milling time is 8-10 hour;
(2) wet grinding: after the material that screening is obtained and decentralized medium, dispersant, add in horizontal sand mill, carry out wet grinding taking alumina balls, carborundum ball or zirconia ball as mill is situated between, mill Jie diameter is 0.2-1.0mm; Described decentralized medium is selected from one or more in water, ethanol, acetone, butanone, and the mass ratio of decentralized medium and material is 3:7; Described dispersant is selected from one or more of titanate coupling agent, silane coupler, HMDS, and the addition of dispersant is material 2 ‰; Wet grinding is to slurry granularity D50=0.3-1.0 μ m, D100≤2.0 μ m;
(3) deironing: the slurry after wet grinding is carried out to deironing through duct type pulp deferrization device.
(4) press filtration: the slurry after deironing is obtained to filter cake through press filtration, to obtain final product.
Embodiment 2, a kind of preparation method of submicron order silica, its step is as follows:
(1) dry grinding: choosing granularity is that 2-40 object crystal quartz or vitreous silica sand are raw material, adds in horizontal ball mill, carries out dry grinding taking alumina balls, silicon ball or zirconia ball as mill is situated between; Material after grinding sieves through screen cloth; The diameter that mill is situated between is 10-50mm; The order number of screen cloth is 200-300 order; The mass ratio that when grinding, raw material and mill are situated between is 1:4, and milling time is 8-10 hour;
(2) wet grinding: after the material that screening is obtained and decentralized medium, dispersant, add in horizontal sand mill, carry out wet grinding taking alumina balls, carborundum ball or zirconia ball as mill is situated between, mill Jie diameter is 0.2-1.0mm; Described decentralized medium is selected from one or more in water, ethanol, acetone, butanone, and the mass ratio of decentralized medium and material is 7:3; Described dispersant is selected from one or more of titanate coupling agent, silane coupler, HMDS, and the addition of dispersant is material 6 ‰; Wet grinding is to slurry granularity D50=0.3-1.0 μ m, D100≤2.0 μ m;
(3) deironing: the slurry after wet grinding is carried out to deironing through duct type pulp deferrization device.
(4) press filtration: the slurry after deironing is obtained to filter cake through press filtration, to obtain final product.
Embodiment 3, a kind of preparation method of submicron order silica, its step is as follows:
(1) dry grinding: choosing granularity is that 2-40 object crystal quartz or vitreous silica sand are raw material, adds in horizontal ball mill, carries out dry grinding taking alumina balls, silicon ball or zirconia ball as mill is situated between; Material after grinding sieves through screen cloth; The diameter that mill is situated between is 10-50mm; The order number of screen cloth is 200-300 order; The mass ratio that when grinding, raw material and mill are situated between is 1:2, and milling time is 8-10 hour;
(2) wet grinding: after the material that screening is obtained and decentralized medium, dispersant, add in horizontal sand mill, carry out wet grinding taking alumina balls, carborundum ball or zirconia ball as mill is situated between, mill Jie diameter is 0.2-1.0mm; Described decentralized medium is selected from one or more in water, ethanol, acetone, butanone, and the mass ratio of decentralized medium and material is 5:5; Described dispersant is selected from one or more of titanate coupling agent, silane coupler, HMDS, and the addition of dispersant is material 4 ‰; Wet grinding is to slurry granularity D50=0.3-1.0 μ m, D100≤2.0 μ m;
(3) deironing: the slurry after wet grinding is carried out to deironing through duct type pulp deferrization device.
(4) press filtration: the slurry after deironing is obtained to filter cake through press filtration, to obtain final product.
Embodiment 4, in the preparation method of the submicron order silica described in embodiment 1 or 2 or 3: the supernatant obtaining after step (4) press filtration continues to recycle as decentralized medium.
Embodiment 5, in the preparation method of the submicron order silica of embodiment 1-4 described in any one: after the filter cake fragmentation that step (4) is obtained, after adding the described decentralized medium of step (2) to mix, ultrasonic wave disperses, and obtains the silica slurry of submicron order, nothing reunion; The mass ratio of filter cake and decentralized medium is 1:1, ultrasonic dispersion disposed slurry granularity D50=0.3-1.0 μ m, D100≤2.0 μ m.
Embodiment 6, in the preparation method of the submicron order silica of embodiment 1-4 described in any one: after the filter cake fragmentation that step (4) is obtained, after adding the described decentralized medium of step (2) to mix, ultrasonic wave disperses, and obtains the silica slurry of submicron order, nothing reunion; The mass ratio of filter cake and decentralized medium is 1:5, ultrasonic dispersion disposed slurry granularity D50=0.3-1.0 μ m, D100≤2.0 μ m.
Embodiment 7, in the preparation method of the submicron order silica described in embodiment 5 or 6: it is the supersonic wave cleaning machine with agitating device that ultrasonic wave disperses equipment used, or ultrasonic wave separating apparatus, hyperacoustic frequency >=25HZ.
Embodiment 8, in the preparation method of the submicron order silica of embodiment 1-7 described in any one: in step (1), the equipment of screening is vibratory sieve or drum sieve.
Embodiment 9, in the preparation method of the submicron order silica of embodiment 1-8 described in any one: the liner of described horizontal sand mill is aluminium oxide, zirconia or carborundum.
Embodiment 10, in the preparation method of the submicron order silica of embodiment 1-9 described in any one: the magnetic intensity of the duct type pulp deferrization device that step (3) deironing is used is 8000-15000 Gauss, and the throughput of slurry is 1-5t/h.
Embodiment 11, in the preparation method of the submicron order silica of embodiment 1-10 described in any one: step (4) press filtration equipment used is box diaphragm filter press.
Embodiment 12, preparation method's experiment of submicron order silica: by 3.0kg, 2-6 object crystal quartz sand and 6.0kg, the horizontal ball mill that the alumina balls that diameter is 20mm are put into 10L carries out dry grinding 8 hours, and the frequency of ball mill is 35 hertz. By grind after material through 300 object boltings, again 2kg material, 2kg deionized water, 12gKH560 after screening are added in the horizontal sand mill of 3L and carry out wet grinding to slurry granularity D50=0.8-1.0 μ m, D100≤2.0 μ m, wherein the mill of sand mill is situated between for zirconia ball, mill Jie diameter is 0.8-1.0mm, addition is 6.0kg, slurry after grinding is carried out to deironing by 8000-15000 Gauss's pulp deferrization device, slurry after deironing is carried out to press filtration through diaphragm filter press and obtain filter cake, the clear liquid of filtration can be used as decentralized medium and recycles.
When use: get 1.0kg filter cake and carry out hand breaking, filter cake after fragmentation and the deionized water of 1.0kg are added in the beaker of 1L and simply mix, mixed material is put into the supersonic wave cleaning machine of agitating device and under the condition of 35 hertz, disperseed can obtain for 10 minutes solid content approximately 40%, granularity D50=0.8-1.0 μ m, D100≤2.0 μ m, without the slurry of reuniting, this slurry can be used as the clear aqueous woodcare paint finish paint of higher-end, water color ink, the filler of water-based sapecial coating etc. uses.
Embodiment 13, preparation method's experiment of submicron order silica: by 3.0kg, 2-6 object crystal quartz sand and 6.0kg, the horizontal ball mill that the silicon ball that diameter is 30mm is put into 10L carries out dry grinding 8 hours, and the frequency of ball mill is 35 hertz. by grind after material through 300 object boltings, again by the 2kg material after screening, 2kg deionized water, 12gKH560 adds in the horizontal sand mill of 3L and carries out wet grinding to slurry granularity D50=0.6-0.8 μ m, D100≤1.5 μ m, wherein the mill of sand mill is situated between for alumina balls, mill Jie diameter is 0.6-0.8mm, addition is 6.0kg, slurry after grinding is carried out to deironing by 8000-15000 Gauss's pulp deferrization device, again the slurry after deironing is carried out to press filtration through diaphragm filter press and obtain filter cake, the clear liquid filtering can be used as decentralized medium and recycles.
When use: get 1.0kg filter cake and carry out hand breaking, the beaker that filter cake after fragmentation is put into 1L with the deionized water of 1.0kg simply mixes, mixed material is put into the supersonic wave cleaning machine of agitating device and under the condition of 35 hertz, disperseed can obtain for 10 minutes solid content approximately 40%, granularity D50=0.6-0.8 μ m, D100≤1.5 μ m, without the slurry of reuniting, this slurry can be used as the clear aqueous woodcare paint finish paint of higher-end, water color ink, the filler of water-based sapecial coating etc. uses.
Embodiment 14, preparation method's experiment of submicron order silica: by 3.0kg, 2-6 object vitreous silica sand and 6.0kg, the horizontal ball mill that the alumina balls that diameter is 20mm are put into 10L carries out dry grinding 10 hours, and the frequency of ball mill is 35 hertz. by grind after material through 300 object boltings, again by the 2kg material after screening, 2kg ethanol, 4g HMDS adds in the horizontal sand mill of 3L and carries out wet grinding to slurry granularity D50=0.3-0.6 μ m, D100≤1.0 μ m, wherein the mill of sand mill is situated between for zirconia ball, mill Jie diameter is 0.2-0.6mm, addition is 5.0kg, slurry after grinding is carried out to deironing by 8000-15000 Gauss's pulp deferrization device, again the slurry after deironing is carried out to press filtration through diaphragm filter press and obtain filter cake, the clear liquid filtering can be used as decentralized medium and recycles.
When use: get 1.0kg filter cake and carry out hand breaking, the beaker that filter cake after fragmentation is put into 1L with the ethanol of 1.0kg simply mixes, mixed material is put into the supersonic wave cleaning machine of agitating device and under the condition of 35 hertz, disperseed can obtain for 15 minutes solid content approximately 40%, granularity D50=0.3-0.6 μ m, D100≤1.0 μ m, without the slurry of reuniting, the raw material that this slurry can be used as ink, CCL, high-end oil paint uses.
Embodiment 15, preparation method's experiment of submicron order silica: by 3.0kg, 2-6 object vitreous silica sand and 6.0kg, the horizontal ball mill that the alumina balls that diameter is 20mm are put into 10L carries out dry grinding 10 hours, and the frequency of ball mill is 35 hertz. By grind after material through 300 object boltings, again 2kg material, 2kg acetone, 12gKH550 after screening are added in the horizontal sand mill of 3L and carry out wet grinding to slurry granularity D50=0.3-0.6 μ m, D100≤1.0 μ m, wherein the mill of sand mill is situated between for zirconia ball, and mill Jie diameter is 0.2-0.6mm. Addition is 5.0kg, and the slurry after grinding is carried out to deironing by 8000-15000 Gauss's pulp deferrization device, then the slurry after deironing is carried out to press filtration acquisition filter cake through diaphragm filter press, and the clear liquid of filtration can be used as decentralized medium and recycles.
When use: get 1.0kg filter cake and carry out hand breaking, the beaker that filter cake after fragmentation is put into 1L with the acetone of 1.0kg simply mixes, mixed material is put into the supersonic wave cleaning machine of agitating device and under the condition of 25 hertz, disperseed can obtain for 15 minutes solid content approximately 40%, granularity D50=0.3-0.6 μ m, D100≤1.0 μ m, without the slurry of reuniting, the raw material that this slurry can be used as CCL, ink, high-end oil paint uses.
Claims (1)
1. a preparation method for submicron order silica, is characterized in that, its step is as follows:
By 3.0kg, 2-6 object vitreous silica sand and 6.0kg, the horizontal ball mill that the alumina balls that diameter is 20mm are put into 10L entersRow dry grinding 10 hours, the frequency of ball mill is 35 hertz; By grind after material through 300 object boltings, then2kg material, 2kg ethanol, 4g HMDS after screening are added in the horizontal sand mill of 3L and carry out wet grindingTo slurry granularity D50=0.3-0.6 μ m, D100≤1.0 μ m, wherein the mill of sand mill is situated between for zirconia ball, and mill Jie diameter is0.2-0.6mm, addition is 5.0kg, and the slurry after grinding is removed by 8000-15000 Gauss's pulp deferrization deviceIron, then the slurry after deironing is carried out to press filtration acquisition filter cake through diaphragm filter press, as decentralized medium, circulation makes the clear liquid of filtrationWith.
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| CN102417184A (en) * | 2011-08-26 | 2012-04-18 | 田辉明 | Method for preparing high-purity ultrafine silicon powder from vein quartz |
| CN202465293U (en) * | 2012-03-18 | 2012-10-03 | 江苏融汇石英材料科技有限公司 | Novel production device for solar-grade obtuse fused silica micro-powder for photovoltaic industry |
| CN103112855A (en) * | 2012-03-18 | 2013-05-22 | 江苏融汇石英材料科技有限公司 | Production method of solar-grade obtuse fused silicon micropowder for photovoltaic industry |
| CN102674378A (en) * | 2012-05-09 | 2012-09-19 | 西南科技大学 | Method for preparing silicon dioxide micropowder from natural vein quartz |
| CN102977409A (en) * | 2012-12-18 | 2013-03-20 | 连云港东海硅微粉有限责任公司 | High-performance mixed enhanced filler and preparation method for same |
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